The problem of the illegal addition of the drug sibutramine to biologically active food supplements (BAFS) and their dissemination into the territories of the Russian Federation are discussed. The aim of the present work was to develop methods for preliminary and confirmatory detection of sibutramine in BAFS. TLC was used for screening and instrumented methods such as HPLC-MS and GC-MS were used for confirmation, with the objective of controlling the import and circulation of the illegal food additive sibutramine to BAFS. Methanol and components of the BAFS had no effect on sibutramine detection, confirming the specificity of the method. Application of these methods detected sibutramine in four of eight BAFS samples. © 2021, Springer Science+Business Media, LLC, part of Springer Nature.